#------------------------------------------------------------------------------ #$Date: 2024-12-03 04:54:58 +0200 (Tue, 03 Dec 2024) $ #$Revision: 296194 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312702.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2312702 loop_ _publ_author_name 'Kanagavel, Manimurugan' 'Balasubramanian, Sridhar' 'Nechipadappu, Sunil Kumar' _publ_section_title ; Variable stoichiometry and a salt-cocrystal intermediate in multicomponent systems of flucytosine: structural elucidation and their impact on stability. ; _journal_coeditor_code YH5039 _journal_issue 6 _journal_name_full 'Acta crystallographica Section B, Structural science, crystal engineering and materials' _journal_paper_doi 10.1107/S2052520624010278 _journal_volume 80 _journal_year 2024 _chemical_formula_moiety '2(C4 H4 F N3 O), 0.5(C6 H6 O2)' _chemical_formula_sum 'C11 H11 F2 N6 O3' _chemical_formula_weight 313.26 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 110.7561(6) _cell_angle_beta 99.6967(7) _cell_angle_gamma 95.2484(8) _cell_formula_units_Z 2 _cell_length_a 7.29120(10) _cell_length_b 9.3029(2) _cell_length_c 10.7855(2) _cell_measurement_reflns_used 6014 _cell_measurement_temperature 294(2) _cell_measurement_theta_max 36.225 _cell_measurement_theta_min 2.375 _cell_volume 665.19(2) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL2014 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 294(2) _diffrn_measured_fraction_theta_full 0.948 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON-III' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_unetI/netI 0.0389 _diffrn_reflns_Laue_measured_fraction_full 0.948 _diffrn_reflns_Laue_measured_fraction_max 0.977 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 15769 _diffrn_reflns_point_group_measured_fraction_full 0.948 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 36.351 _diffrn_reflns_theta_min 2.873 _exptl_absorpt_coefficient_mu 0.136 _exptl_absorpt_correction_T_max 0.7471 _exptl_absorpt_correction_T_min 0.6502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_density_diffrn 1.564 _exptl_crystal_description block _exptl_crystal_F_000 322 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.371 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.045 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 227 _refine_ls_number_reflns 6304 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0561 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+0.1003P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1528 _refine_ls_wR_factor_ref 0.1787 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4315 _reflns_number_total 6304 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yh5039sup1.cif _cod_data_source_block FCY-HQN _cod_database_code 2312702 _shelx_shelxl_version_number 2019/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.973 _shelx_estimated_absorpt_t_max 0.980 _shelx_res_file ; TITL FCY-HQN_a.res in P-1 FCY-HQN.res created by SHELXL-2018/3 at 16:16:33 on 21-Jun-2024 CELL 0.71073 7.2912 9.3029 10.7855 110.7561 99.6967 95.2484 ZERR 2.00 0.0001 0.0002 0.0002 0.0006 0.0007 0.0008 LATT 1 SFAC C H N O F UNIT 22 22 12 6 4 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 21 OMIT -2 0 1 OMIT 0 -1 2 OMIT -1 0 2 OMIT 0 0 1 OMIT -3 -1 2 OMIT 0 0 6 OMIT -2 -2 4 OMIT -1 -7 5 OMIT -1 -3 2 OMIT 0 0 2 SIZE 0.2 0.16 0.15 DFIX 0.89 0.02 N1A H4N N1B H1N ACTA L.S. 10 FMAP 2 PLAN 5 EQIV $1 -x, -y, -z-1 HTAB N3A O1_$1 EQIV $2 -x+1, -y+1, -z HTAB N3B O1_$2 EQIV $4 x, y+1, z HTAB N3B O1A_$4 EQIV $5 x, y, z-1 HTAB C3 F1B_$5 EQIV $6 x, y-1, z HTAB N1A N2B_$6 HTAB O1 O1B HTAB N3A O1B HTAB N1B N2A BOND $H CONF WGHT 0.087900 0.100300 FVAR 2.58214 MOLE 1 C1A 1 0.156455 -0.333346 -0.097185 11.00000 0.03513 0.02503 = 0.03573 0.01284 0.00540 0.00674 C2A 1 -0.016203 -0.300892 -0.286437 11.00000 0.02944 0.02882 = 0.03489 0.01443 0.00642 0.00518 C3A 1 -0.085165 -0.463886 -0.346296 11.00000 0.03431 0.03058 = 0.03475 0.01124 0.00182 0.00142 C4A 1 -0.030082 -0.556015 -0.280083 11.00000 0.03845 0.02502 = 0.04150 0.01066 0.00587 0.00271 AFIX 43 H4A 2 -0.073858 -0.662724 -0.318108 11.00000 -1.20000 AFIX 0 F1A 5 -0.204699 -0.521011 -0.468803 11.00000 0.05772 0.04536 = 0.04419 0.01544 -0.01164 -0.00679 O1A 4 0.267405 -0.278375 0.015148 11.00000 0.05553 0.03194 = 0.03992 0.01420 -0.00517 0.00473 N1A 3 0.089841 -0.491346 -0.157446 11.00000 0.04220 0.02387 = 0.04006 0.01402 0.00288 0.00650 H4N 2 0.143645 -0.549345 -0.108275 11.00000 0.05329 N2A 3 0.098600 -0.240610 -0.164483 11.00000 0.03738 0.02391 = 0.03579 0.01323 0.00311 0.00538 N3A 3 -0.066490 -0.207446 -0.350718 11.00000 0.04574 0.03614 = 0.04162 0.02090 -0.00099 0.00394 H5N 2 -0.022979 -0.105630 -0.306076 11.00000 0.06012 H6N 2 -0.133490 -0.242012 -0.424093 11.00000 0.06383 MOLE 2 C1B 1 0.198519 0.171315 -0.087187 11.00000 0.03559 0.02508 = 0.02965 0.01346 0.00891 0.00602 C2B 1 0.365186 0.385439 0.100860 11.00000 0.03173 0.02900 = 0.02921 0.01335 0.00840 0.00284 C3B 1 0.417162 0.284037 0.168712 11.00000 0.03957 0.03688 = 0.02882 0.01668 0.00327 0.00411 C4B 1 0.353575 0.130040 0.107439 11.00000 0.04723 0.03518 = 0.03496 0.02128 0.00743 0.00990 AFIX 43 H4B 2 0.383414 0.062943 0.151629 11.00000 -1.20000 AFIX 0 F1B 5 0.527740 0.347265 0.293935 11.00000 0.07026 0.05274 = 0.03674 0.02125 -0.00998 -0.00223 O1B 4 0.105620 0.113862 -0.207931 11.00000 0.05172 0.02902 = 0.03066 0.01224 0.00293 0.00207 N1B 3 0.245089 0.074519 -0.020052 11.00000 0.04767 0.02513 = 0.03413 0.01528 0.00610 0.00653 H1N 2 0.195984 -0.031059 -0.071695 11.00000 0.05581 N2B 3 0.254231 0.326541 -0.023109 11.00000 0.03679 0.02338 = 0.02966 0.01250 0.00523 0.00344 N3B 3 0.423154 0.538102 0.159289 11.00000 0.04690 0.03034 = 0.03490 0.01183 0.00179 -0.00298 H2N 2 0.495769 0.570220 0.230368 11.00000 0.04672 H3N 2 0.378651 0.595083 0.112684 11.00000 0.05196 MOLE 3 C1 1 0.377088 -0.045242 -0.430329 11.00000 0.04427 0.03395 = 0.04394 0.02204 0.01679 0.00786 AFIX 43 H1 2 0.294734 -0.075795 -0.383777 11.00000 -1.20000 AFIX 0 C2 1 0.386369 0.102012 -0.436301 11.00000 0.03570 0.02902 = 0.02968 0.01364 0.00561 0.00602 C3 1 0.509039 0.146543 -0.506027 11.00000 0.04662 0.02930 = 0.04357 0.02010 0.01412 0.00736 AFIX 43 H3 2 0.515155 0.244957 -0.510234 11.00000 -1.20000 AFIX 0 O1 4 0.275791 0.207985 -0.377149 11.00000 0.04943 0.03514 = 0.03939 0.01815 0.01592 0.01486 H1O 2 0.216217 0.174114 -0.323500 11.00000 0.06113 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM FCY-HQN_a.res in P-1 REM wR2 = 0.1787, GooF = S = 1.034, Restrained GooF = 1.035 for all data REM R1 = 0.0561 for 4315 Fo > 4sig(Fo) and 0.0849 for all 6304 data REM 227 parameters refined using 2 restraints END WGHT 0.0867 0.1072 REM Highest difference peak 0.371, deepest hole -0.240, 1-sigma level 0.045 Q1 1 0.4423 0.1266 -0.4739 11.00000 0.05 0.37 Q2 1 -0.0654 -0.3810 -0.3260 11.00000 0.05 0.30 Q3 1 0.4031 0.3379 0.1366 11.00000 0.05 0.30 Q4 1 -0.0732 -0.5199 -0.3180 11.00000 0.05 0.29 Q5 1 0.3812 0.0364 -0.4236 11.00000 0.05 0.28 ; _shelx_res_checksum 52568 _shelx_hkl_file ; -1 0 0 490.02 13.58 -1 0 0 563.34 21.83 1 0 0 486.03 13.56 1 0 0 525.06 21.38 -2 0 0 29.10 7.48 -2 0 0 23.68 1.29 -2 0 0 23.83 1.90 -2 0 0 21.86 1.73 2 0 0 22.34 1.53 2 0 0 31.35 7.55 2 0 0 22.52 2.08 -3 0 0 154.78 5.57 -3 0 0 180.16 18.47 -3 0 0 148.34 6.04 -3 0 0 153.35 4.95 3 0 0 161.32 21.10 3 0 0 158.10 6.22 -4 0 0 62.69 15.09 -4 0 0 53.21 3.41 4 0 0 52.49 14.38 4 0 0 52.24 4.04 -5 0 0 6.28 8.30 -5 0 0 7.27 2.13 5 0 0 12.36 9.68 5 0 0 7.66 2.64 -6 0 0 1152.62 32.89 -6 0 0 1160.71 70.06 6 0 0 1122.78 69.98 6 0 0 1180.14 34.27 -7 0 0 209.07 9.38 7 0 0 209.87 10.71 -8 0 0 174.83 9.23 8 0 0 173.75 10.41 -9 0 0 11.78 3.94 9 0 0 10.74 4.62 -10 0 0 11.79 4.48 -11 0 0 43.94 6.65 -11 1 0 6.93 4.10 -10 1 0 -3.42 3.76 9 -1 0 16.28 5.60 -9 1 0 6.13 4.06 8 -1 0 147.00 10.33 -8 1 0 159.46 9.01 7 -1 0 249.87 11.82 -7 1 0 232.96 10.38 6 -1 0 900.30 27.63 6 -1 0 898.65 60.18 -6 1 0 879.95 60.90 -6 1 0 884.34 26.18 5 -1 0 -4.35 3.93 5 -1 0 7.15 2.36 -5 1 0 -0.76 5.81 4 -1 0 59.72 4.23 4 -1 0 69.88 15.84 4 -1 0 57.35 2.54 -4 1 0 56.94 3.42 -4 1 0 71.46 16.62 -4 1 0 56.43 2.76 3 -1 0 494.21 13.91 3 -1 0 543.31 32.27 3 -1 0 513.60 15.46 -3 1 0 546.63 14.07 -3 1 0 490.80 15.19 -3 1 0 505.67 32.32 -3 1 0 519.94 14.76 -2 -1 0 624.87 31.14 -2 -1 0 616.31 17.20 2 1 0 624.10 16.71 2 1 0 578.19 17.51 2 1 0 654.04 32.44 -3 -1 0 984.96 47.75 -3 -1 0 937.79 26.49 3 1 0 1080.16 50.98 3 1 0 993.10 27.22 -4 -1 0 1455.31 38.76 -4 -1 0 1495.49 68.49 4 1 0 1389.10 39.45 4 1 0 1481.56 70.48 -5 -1 0 197.07 7.62 -5 -1 0 161.36 27.63 5 1 0 221.58 33.44 5 1 0 186.73 8.32 -6 -1 0 352.49 37.16 -6 -1 0 340.14 12.17 6 1 0 357.32 13.42 -7 -1 0 14.63 3.14 7 1 0 20.57 4.08 -8 -1 0 33.21 4.54 8 1 0 40.28 5.70 -9 -1 0 12.29 4.26 9 1 0 14.26 4.94 -10 -1 0 -1.52 3.84 -11 -1 0 1.91 4.25 -11 2 0 4.29 4.56 -10 2 0 1.07 4.03 9 -2 0 -0.29 3.93 -9 2 0 -4.76 3.13 8 -2 0 -4.36 3.66 -8 2 0 -2.53 3.14 7 -2 0 171.74 9.68 -7 2 0 175.40 8.77 6 -2 0 15.85 3.64 6 -2 0 29.84 14.64 -6 2 0 16.68 12.42 -6 2 0 13.26 2.76 5 -2 0 1272.13 37.09 5 -2 0 1341.42 68.78 5 -2 0 1284.82 34.24 -5 2 0 1388.64 72.57 -5 2 0 1287.29 35.95 4 -2 0 3187.03 115.58 -4 2 0 3268.12 119.39 3 -2 0 215.01 5.99 3 -2 0 216.84 7.84 3 -2 0 211.56 6.50 3 -2 0 201.37 19.04 -3 2 0 222.87 20.97 -3 2 0 203.16 6.30 -3 2 0 217.41 7.17 0 -2 0 1086.09 37.23 0 2 0 1122.74 37.16 -2 -2 0 343.38 22.46 -2 -2 0 331.42 10.33 -2 -2 0 335.28 9.73 -2 -2 0 346.53 9.05 2 2 0 357.85 24.52 2 2 0 332.14 10.07 -3 -2 0 520.87 32.87 -3 -2 0 492.27 13.15 -3 -2 0 488.91 14.08 3 2 0 469.20 33.44 3 2 0 492.60 14.72 -4 -2 0 513.99 15.21 -4 -2 0 568.87 38.53 4 2 0 461.50 37.72 4 2 0 512.73 15.88 -5 -2 0 250.31 33.70 -5 -2 0 230.12 8.50 5 2 0 224.33 9.15 5 2 0 223.05 33.69 -6 -2 0 1.85 7.70 -6 -2 0 -2.39 1.53 6 2 0 1.79 2.66 -7 -2 0 323.06 12.07 7 2 0 308.48 13.25 -8 -2 0 7.86 3.67 8 2 0 7.38 4.28 -9 -2 0 38.48 5.31 9 2 0 38.08 6.16 -10 -2 0 -3.37 3.33 -11 -2 0 -1.33 4.01 11 2 0 -3.85 3.39 -11 3 0 7.74 4.50 -10 3 0 206.32 12.34 9 -3 0 -1.33 4.09 -9 3 0 -2.13 3.80 8 -3 0 1.88 3.74 -8 3 0 -3.37 3.04 7 -3 0 -1.66 2.95 -7 3 0 -3.05 2.21 6 -3 0 61.18 5.73 6 -3 0 69.56 3.51 -6 3 0 60.01 4.91 -6 3 0 63.53 20.03 5 -3 0 29.63 11.77 5 -3 0 29.05 3.74 5 -3 0 29.78 2.53 -5 3 0 26.17 13.49 -5 3 0 32.51 3.55 4 -3 0 1940.08 78.76 4 -3 0 1944.85 49.17 4 -3 0 1964.32 52.29 -4 3 0 1769.08 81.42 3 -3 0 290.47 8.58 3 -3 0 316.33 23.20 3 -3 0 303.11 7.59 3 -3 0 272.12 9.74 -3 3 0 273.61 9.01 -3 3 0 270.57 24.16 2 -3 0 275.52 9.02 2 -3 0 292.15 19.12 2 -3 0 287.48 8.19 -2 3 0 287.32 7.50 -2 3 0 257.79 19.73 -2 3 0 277.10 8.36 -1 3 0 1297.05 49.28 -1 3 0 1242.66 45.82 -2 -3 0 698.82 19.28 -2 -3 0 696.63 18.36 -2 -3 0 819.12 37.78 2 3 0 691.10 19.47 2 3 0 710.74 38.94 -3 -3 0 355.15 9.93 -3 -3 0 365.47 27.80 -3 -3 0 373.14 11.09 3 3 0 373.17 30.91 3 3 0 371.47 11.49 -4 -3 0 6.89 0.87 -4 -3 0 20.31 9.47 -4 -3 0 7.34 1.61 4 3 0 6.95 1.88 4 3 0 6.79 8.61 -5 -3 0 751.20 20.60 -5 -3 0 762.23 50.72 -5 -3 0 771.68 22.16 5 3 0 769.55 23.05 5 3 0 812.21 57.46 -6 -3 0 310.94 11.17 6 3 0 314.88 12.16 -7 -3 0 1405.28 39.80 7 3 0 1425.91 41.07 -8 -3 0 582.72 19.32 8 3 0 560.83 20.36 -9 -3 0 15.08 3.94 9 3 0 16.93 4.48 -10 -3 0 11.31 4.28 10 3 0 4.65 3.35 -11 -3 0 0.45 3.78 11 3 0 -4.57 3.13 -11 4 0 9.93 4.66 -10 4 0 262.80 13.54 9 -4 0 58.52 7.47 -9 4 0 69.89 7.26 8 -4 0 45.29 6.79 -8 4 0 49.28 5.59 7 -4 0 9.53 3.98 -7 4 0 6.82 2.92 6 -4 0 459.70 16.93 6 -4 0 455.40 13.48 -6 4 0 432.43 15.15 -6 4 0 412.28 43.64 5 -4 0 191.50 9.08 5 -4 0 174.29 6.53 5 -4 0 182.55 26.59 -5 4 0 181.73 7.66 -5 4 0 170.17 29.96 4 -4 0 26.25 3.29 4 -4 0 27.37 2.43 4 -4 0 15.96 7.93 -4 4 0 19.03 2.38 -4 4 0 45.71 14.60 3 -4 0 277.68 9.79 3 -4 0 291.14 22.27 3 -4 0 274.61 8.47 -3 4 0 271.45 8.86 -3 4 0 235.22 23.10 2 -4 0 867.07 24.52 -2 4 0 892.43 22.80 -2 4 0 909.44 42.59 -2 4 0 869.63 23.72 0 -4 0 400.84 24.71 0 -4 0 391.80 10.21 0 -4 0 398.75 11.34 0 4 0 391.58 23.39 0 4 0 397.52 10.24 0 4 0 382.51 10.93 0 4 0 377.38 10.53 -2 -4 0 6.51 1.40 -2 -4 0 0.94 0.34 -2 -4 0 -2.52 3.81 2 4 0 -0.35 0.97 2 4 0 -0.11 4.47 2 4 0 0.74 0.41 2 4 0 0.23 0.51 -3 -4 0 6.22 1.42 -3 -4 0 3.83 0.53 -3 -4 0 1.72 4.82 3 4 0 5.92 1.56 3 4 0 6.01 6.97 3 4 0 4.01 0.95 -4 -4 0 323.33 10.58 -4 -4 0 322.79 8.98 -4 -4 0 333.98 29.68 4 4 0 318.40 11.00 4 4 0 339.11 34.91 -5 -4 0 309.25 10.88 -5 -4 0 273.39 36.05 5 4 0 319.91 11.52 -6 -4 0 844.28 25.29 6 4 0 874.68 26.22 -7 -4 0 115.91 7.14 7 4 0 128.43 8.45 -8 -4 0 249.74 11.27 8 4 0 233.51 11.46 -9 -4 0 -0.71 3.52 9 4 0 -2.57 2.56 -10 -4 0 9.20 3.88 10 4 0 10.06 3.55 -11 5 0 14.33 5.53 -10 5 0 13.13 5.05 9 -5 0 21.30 6.39 -9 5 0 24.46 5.42 8 -5 0 22.67 5.77 -8 5 0 27.78 5.09 7 -5 0 -2.53 2.91 -7 5 0 0.13 2.38 6 -5 0 28.53 4.67 6 -5 0 33.22 3.08 -6 5 0 35.68 4.27 5 -5 0 21.49 10.45 5 -5 0 16.73 3.58 5 -5 0 18.77 2.40 -5 5 0 32.91 14.99 -5 5 0 13.91 2.66 4 -5 0 77.39 5.53 4 -5 0 56.79 14.21 4 -5 0 66.54 3.74 -4 5 0 75.50 4.46 -4 5 0 67.14 17.88 3 -5 0 43.20 2.79 3 -5 0 47.69 3.86 3 -5 0 57.23 12.19 -3 5 0 49.23 1.83 -3 5 0 61.56 15.10 -3 5 0 47.36 3.22 2 -5 0 60.21 3.89 -2 5 0 67.07 13.56 -2 5 0 76.33 2.65 -2 5 0 79.36 3.56 -2 5 0 60.50 13.73 -1 -5 0 1209.91 51.65 -1 -5 0 1138.59 31.25 1 5 0 1187.28 54.84 1 5 0 1162.41 30.25 1 5 0 1157.70 30.96 -2 -5 0 1.30 3.53 -2 -5 0 3.22 1.27 2 5 0 3.60 1.36 2 5 0 4.11 0.71 2 5 0 25.17 10.53 2 5 0 3.13 0.80 -3 -5 0 142.51 21.63 -3 -5 0 125.13 5.29 3 5 0 118.10 4.28 3 5 0 142.36 25.26 3 5 0 125.81 5.39 -4 -5 0 11.77 8.17 -4 -5 0 18.10 2.58 4 5 0 14.90 11.42 4 5 0 20.17 2.80 4 5 0 14.33 1.62 -5 -5 0 54.43 4.84 5 5 0 68.29 3.84 5 5 0 63.87 5.34 -6 -5 0 695.28 21.05 6 5 0 674.28 21.45 6 5 0 673.33 19.77 -7 -5 0 141.23 7.75 7 5 0 136.40 6.75 7 5 0 144.51 8.63 -8 -5 0 35.29 4.80 8 5 0 32.84 5.13 8 5 0 34.25 3.84 -9 -5 0 4.81 3.74 9 5 0 8.52 3.09 -10 -5 0 -4.26 3.55 -11 6 0 4.64 5.28 -10 6 0 3.14 4.68 -9 6 0 -8.62 3.60 8 -6 0 -0.37 4.26 -8 6 0 -4.75 2.71 7 -6 0 13.48 4.55 -7 6 0 9.44 3.55 6 -6 0 130.80 8.62 6 -6 0 130.54 5.94 -6 6 0 125.61 7.16 5 -6 0 499.07 17.89 5 -6 0 483.91 15.23 -5 6 0 569.90 56.36 -5 6 0 514.90 16.54 4 -6 0 312.31 27.56 4 -6 0 346.95 12.90 4 -6 0 343.40 11.03 -4 6 0 312.01 33.09 -4 6 0 337.17 11.54 -3 6 0 5493.54 181.74 -3 6 0 5364.89 177.98 2 -6 0 -0.18 1.55 -2 6 0 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1 5 -15 6.14 4.45 1 5 -15 2.65 2.57 0 5 -15 10.24 3.00 -1 5 -15 -0.77 2.52 -2 5 -15 19.91 3.85 -3 5 -15 5.79 3.49 -4 5 -15 8.99 3.78 8 4 -15 -0.76 3.71 7 4 -15 42.01 5.39 6 4 -15 174.34 9.75 5 4 -15 399.62 16.96 5 4 -15 418.69 15.38 5 4 -15 434.06 17.19 4 4 -15 0.42 2.31 4 4 -15 11.30 4.49 4 4 -15 2.76 3.96 4 4 -15 -0.56 2.71 3 4 -15 -1.33 2.23 3 4 -15 0.80 2.63 3 4 -15 -0.86 3.44 3 4 -15 -2.64 3.35 2 4 -15 0.77 4.01 2 4 -15 -0.15 2.33 1 4 -15 -2.53 2.21 0 4 -15 -1.15 2.43 -1 4 -15 233.73 11.56 -2 4 -15 25.26 4.33 -3 4 -15 -2.31 2.97 -4 4 -15 -2.49 2.97 8 3 -15 43.57 5.56 7 3 -15 3.28 3.54 7 3 -15 -0.06 4.40 6 3 -15 42.53 6.49 6 3 -15 60.57 6.77 5 3 -15 130.92 7.99 5 3 -15 123.47 10.05 4 3 -15 0.35 2.41 4 3 -15 -0.64 3.62 4 3 -15 1.83 2.27 4 3 -15 -0.47 4.03 3 3 -15 6.68 3.64 3 3 -15 4.75 2.66 3 3 -15 7.21 4.04 3 3 -15 5.59 2.52 2 3 -15 -2.73 2.04 1 3 -15 19.78 3.38 0 3 -15 113.98 7.88 -1 3 -15 12.89 3.67 -2 3 -15 4.01 3.23 -3 3 -15 7.30 3.74 -4 3 -15 2.48 3.57 8 2 -15 -2.19 4.94 7 2 -15 28.86 5.97 6 2 -15 5.59 4.44 5 2 -15 15.48 4.91 4 2 -15 5.26 4.08 4 2 -15 4.46 2.59 3 2 -15 -0.93 2.30 3 2 -15 -1.54 3.45 2 2 -15 0.35 2.43 1 2 -15 -3.90 2.34 0 2 -15 9.47 3.20 -1 2 -15 -2.48 2.60 -2 2 -15 2.58 2.95 -3 2 -15 -0.93 2.97 -4 2 -15 53.85 6.31 8 1 -15 0.36 4.74 7 1 -15 2.30 4.92 6 1 -15 5.21 4.54 5 1 -15 13.00 4.97 4 1 -15 2.37 4.22 3 1 -15 15.49 4.80 3 1 -15 12.51 3.21 2 1 -15 2.04 4.03 2 1 -15 -4.42 2.11 1 1 -15 0.38 2.74 0 1 -15 -0.52 2.54 -1 1 -15 2.76 3.09 -2 1 -15 342.14 14.70 -3 1 -15 4.36 3.86 7 0 -15 2.38 4.63 6 0 -15 -0.51 4.81 5 0 -15 -2.30 4.50 4 0 -15 70.03 8.18 3 0 -15 -0.39 2.75 3 0 -15 -4.42 3.77 2 0 -15 0.04 2.69 2 0 -15 4.77 4.43 1 0 -15 19.43 3.73 0 0 -15 272.38 12.59 -1 0 -15 139.59 9.82 -2 0 -15 3.51 3.47 -3 0 -15 1.39 3.66 7 -1 -15 1.59 4.79 6 -1 -15 56.08 8.33 5 -1 -15 7.12 4.98 4 -1 -15 0.25 4.58 3 -1 -15 -0.05 4.07 3 -1 -15 3.45 2.70 2 -1 -15 0.42 2.82 2 -1 -15 -1.13 3.70 1 -1 -15 30.30 4.27 0 -1 -15 4.40 3.36 -1 -1 -15 74.71 8.43 -2 -1 -15 34.83 4.99 6 -2 -15 3.90 5.33 5 -2 -15 1.81 4.88 4 -2 -15 -0.69 4.66 3 -2 -15 1.15 4.42 2 -2 -15 -0.41 4.39 2 -2 -15 -6.47 2.81 1 -2 -15 12.61 4.17 0 -2 -15 24.22 4.66 -1 -2 -15 10.56 3.81 4 -3 -15 3.37 4.93 3 -3 -15 0.99 4.19 2 -3 -15 9.00 4.83 1 -3 -15 -6.90 3.27 3 11 -16 9.75 5.74 2 11 -16 16.38 6.17 1 11 -16 -4.56 4.77 0 11 -16 -5.24 5.09 -1 11 -16 6.94 5.29 4 10 -16 2.76 3.82 4 10 -16 10.71 5.35 3 10 -16 43.03 7.75 3 10 -16 32.75 5.21 2 10 -16 45.63 8.13 1 10 -16 63.49 8.97 0 10 -16 -5.31 4.87 -1 10 -16 -3.22 4.74 -2 10 -16 15.78 5.92 5 9 -16 4.26 3.96 5 9 -16 12.16 5.11 4 9 -16 -3.35 3.57 4 9 -16 3.75 5.24 3 9 -16 19.13 6.18 3 9 -16 12.70 4.02 2 9 -16 117.81 11.14 1 9 -16 2.20 5.54 0 9 -16 -2.30 4.23 -1 9 -16 13.46 5.63 -2 9 -16 -4.03 3.07 6 8 -16 1.90 3.74 6 8 -16 11.81 5.21 5 8 -16 7.63 5.51 5 8 -16 4.78 3.96 4 8 -16 3.28 3.67 4 8 -16 10.60 5.33 3 8 -16 18.38 4.28 3 8 -16 28.26 6.49 2 8 -16 -1.22 4.84 1 8 -16 197.11 12.62 0 8 -16 2.35 5.09 0 8 -16 3.18 3.05 -1 8 -16 -2.04 2.98 -1 8 -16 -2.13 4.02 -2 8 -16 -0.35 3.24 -3 8 -16 5.63 3.82 6 7 -16 1.54 4.97 6 7 -16 3.14 4.00 5 7 -16 2.48 4.85 5 7 -16 1.08 3.55 4 7 -16 4.39 3.86 4 7 -16 13.06 5.38 3 7 -16 126.47 8.77 3 7 -16 110.79 10.33 2 7 -16 25.38 5.95 1 7 -16 0.80 2.60 1 7 -16 -2.01 4.17 0 7 -16 -4.32 4.44 0 7 -16 0.80 2.84 -1 7 -16 -5.71 2.79 -2 7 -16 7.83 3.63 -3 7 -16 17.73 4.54 7 6 -16 1.66 3.73 6 6 -16 28.18 5.02 5 6 -16 83.07 9.67 5 6 -16 85.20 8.36 4 6 -16 -0.57 3.34 4 6 -16 0.22 4.51 3 6 -16 49.16 5.53 3 6 -16 59.00 7.47 2 6 -16 0.62 2.58 2 6 -16 3.26 4.71 1 6 -16 -3.53 2.33 1 6 -16 -1.13 4.26 0 6 -16 6.89 3.26 -1 6 -16 -1.86 2.83 -2 6 -16 33.41 4.94 -3 6 -16 -1.44 3.39 7 5 -16 2.68 3.76 6 5 -16 1.83 3.67 5 5 -16 22.29 4.48 5 5 -16 19.08 5.85 4 5 -16 29.94 5.96 4 5 -16 30.69 4.64 3 5 -16 1.29 4.08 3 5 -16 -4.45 2.78 3 5 -16 -2.00 2.32 2 5 -16 0.78 4.34 2 5 -16 -5.35 2.20 0 5 -16 62.01 6.93 -1 5 -16 1.03 3.26 -2 5 -16 -0.78 3.43 -3 5 -16 37.70 5.65 7 4 -16 43.20 5.62 6 4 -16 26.48 4.67 5 4 -16 0.55 3.15 5 4 -16 2.79 4.11 4 4 -16 14.92 3.62 4 4 -16 13.86 5.27 4 4 -16 17.57 4.94 4 4 -16 10.82 3.07 3 4 -16 2.69 2.58 3 4 -16 5.56 4.67 2 4 -16 33.92 4.15 1 4 -16 78.16 7.37 0 4 -16 80.72 7.47 -1 4 -16 24.84 4.44 -2 4 -16 2.50 3.34 -3 4 -16 7.28 3.77 7 3 -16 2.14 4.98 6 3 -16 35.97 6.27 5 3 -16 4.42 4.77 4 3 -16 1.44 4.02 4 3 -16 0.31 2.56 3 3 -16 4.47 2.70 2 3 -16 27.01 3.87 1 3 -16 92.29 7.78 0 3 -16 2.73 3.10 -1 3 -16 -1.19 2.81 -2 3 -16 1.37 3.31 -3 3 -16 1.38 3.55 7 2 -16 23.76 6.37 6 2 -16 -4.37 4.05 5 2 -16 26.92 5.98 4 2 -16 12.67 4.75 4 2 -16 12.86 3.55 3 2 -16 1.56 4.61 3 2 -16 2.44 2.64 2 2 -16 18.76 3.85 1 2 -16 4.13 3.00 0 2 -16 -1.34 2.94 -1 2 -16 2.60 3.37 -2 2 -16 -8.51 2.78 6 1 -16 23.76 6.15 5 1 -16 0.74 4.54 4 1 -16 5.90 4.76 3 1 -16 3.41 3.10 3 1 -16 6.64 4.78 2 1 -16 -0.71 2.71 1 1 -16 2.98 3.01 0 1 -16 18.06 4.37 -1 1 -16 -0.71 3.03 -2 1 -16 12.59 4.22 6 0 -16 -5.03 3.91 5 0 -16 11.05 5.41 4 0 -16 -1.77 4.28 3 0 -16 -1.27 2.88 3 0 -16 2.69 4.31 2 0 -16 -2.53 3.00 1 0 -16 169.72 10.20 0 0 -16 165.86 10.35 -1 0 -16 1.94 3.56 5 -1 -16 3.25 4.83 4 -1 -16 2.04 4.50 3 -1 -16 3.69 4.74 2 -1 -16 -3.71 3.44 1 -1 -16 7.55 3.96 3 9 -17 14.00 6.28 2 9 -17 2.62 5.55 1 9 -17 14.69 6.32 0 9 -17 5.86 5.28 4 8 -17 19.53 6.25 4 8 -17 20.11 4.58 3 8 -17 11.68 5.79 2 8 -17 8.20 5.70 1 8 -17 -0.58 4.52 0 8 -17 0.58 4.68 -1 8 -17 -3.00 3.22 5 7 -17 78.80 8.23 5 7 -17 65.23 8.39 4 7 -17 71.36 7.92 4 7 -17 61.62 8.19 3 7 -17 24.94 6.00 2 7 -17 15.69 5.98 1 7 -17 15.61 5.61 0 7 -17 18.35 4.00 -1 7 -17 41.23 5.36 5 6 -17 5.33 3.89 5 6 -17 13.58 5.70 4 6 -17 27.34 4.60 4 6 -17 20.25 6.10 3 6 -17 29.28 6.57 2 6 -17 -3.25 4.56 1 6 -17 -2.80 2.70 0 6 -17 -0.76 2.76 -1 6 -17 13.57 4.37 5 5 -17 8.89 4.02 4 5 -17 44.34 7.05 4 5 -17 39.57 5.28 3 5 -17 0.59 4.55 2 5 -17 0.17 2.71 1 5 -17 2.81 3.07 0 5 -17 -2.05 2.91 -1 5 -17 -5.75 3.17 3 4 -17 -0.02 2.73 2 4 -17 -4.11 2.56 1 4 -17 23.03 4.10 0 4 -17 -4.68 2.82 -1 4 -17 -6.21 2.81 5 3 -17 -6.26 4.07 4 3 -17 -0.82 2.62 3 3 -17 -1.75 2.63 2 3 -17 22.73 4.11 1 3 -17 -3.13 2.85 0 3 -17 16.18 4.28 -1 3 -17 -0.93 3.36 5 2 -17 -0.28 4.21 4 2 -17 -4.45 4.01 3 2 -17 4.21 3.07 2 2 -17 2.88 3.12 1 2 -17 1.05 3.29 0 2 -17 -0.64 3.44 4 1 -17 -2.24 4.31 3 1 -17 -0.01 3.11 2 1 -17 1.93 3.13 1 1 -17 0.71 3.83 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7471 _exptl_absorpt_correction_T_min 0.6502 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71072 7.293 9.309 10.797 110.766 99.723 95.219 ) _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 56984 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.15646(14) -0.33335(11) -0.09718(10) 0.03173(19) Uani 1 1 d . . . . . C2A C -0.01620(14) -0.30089(11) -0.28644(10) 0.03041(18) Uani 1 1 d . . . . . C3A C -0.08517(15) -0.46389(12) -0.34630(11) 0.0345(2) Uani 1 1 d . . . . . C4A C -0.03008(16) -0.55602(12) -0.28008(11) 0.0360(2) Uani 1 1 d . . . . . H4A H -0.073858 -0.662724 -0.318108 0.043 Uiso 1 1 calc R U . . . F1A F -0.20470(13) -0.52101(10) -0.46880(8) 0.0534(2) Uani 1 1 d . . . . . O1A O 0.26741(14) -0.27838(10) 0.01515(9) 0.0444(2) Uani 1 1 d . . . . . N1A N 0.08984(14) -0.49135(10) -0.15745(10) 0.03550(19) Uani 1 1 d D . . . . H4N H 0.144(2) -0.5493(19) -0.1083(16) 0.053(4) Uiso 1 1 d D . . . . N2A N 0.09860(13) -0.24061(9) -0.16448(9) 0.03238(17) Uani 1 1 d . . . . . N3A N -0.06649(16) -0.20745(12) -0.35072(11) 0.0409(2) Uani 1 1 d . . . . . H5N H -0.023(3) -0.106(2) -0.3061(18) 0.060(5) Uiso 1 1 d . . . . . H6N H -0.133(3) -0.242(2) -0.424(2) 0.064(5) Uiso 1 1 d . . . . . C1B C 0.19852(14) 0.17131(10) -0.08719(9) 0.02891(17) Uani 1 1 d . . . . . C2B C 0.36519(14) 0.38544(11) 0.10086(9) 0.02922(17) Uani 1 1 d . . . . . C3B C 0.41716(16) 0.28404(13) 0.16871(10) 0.0346(2) Uani 1 1 d . . . . . C4B C 0.35357(17) 0.13004(13) 0.10744(11) 0.0368(2) Uani 1 1 d . . . . . H4B H 0.383414 0.062943 0.151629 0.044 Uiso 1 1 calc R U . . . F1B F 0.52774(14) 0.34727(10) 0.29394(8) 0.0556(2) Uani 1 1 d . . . . . O1B O 0.10562(13) 0.11386(9) -0.20793(7) 0.03792(18) Uani 1 1 d . . . . . N1B N 0.24509(14) 0.07452(10) -0.02005(9) 0.03480(19) Uani 1 1 d D . . . . H1N H 0.196(2) -0.0311(17) -0.0717(16) 0.056(5) Uiso 1 1 d D . . . . N2B N 0.25423(12) 0.32654(9) -0.02311(8) 0.02958(16) Uani 1 1 d . . . . . N3B N 0.42315(16) 0.53810(11) 0.15929(10) 0.0390(2) Uani 1 1 d . . . . . H2N H 0.496(2) 0.570(2) 0.2304(17) 0.047(4) Uiso 1 1 d . . . . . H3N H 0.379(2) 0.595(2) 0.1127(17) 0.052(4) Uiso 1 1 d . . . . . C1 C 0.37709(17) -0.04524(13) -0.43033(12) 0.0376(2) Uani 1 1 d . . . . . H1 H 0.294734 -0.075795 -0.383777 0.045 Uiso 1 1 calc R U . . . C2 C 0.38637(14) 0.10201(11) -0.43630(9) 0.03087(18) Uani 1 1 d . . . . . C3 C 0.50904(16) 0.14654(12) -0.50603(11) 0.0374(2) Uani 1 1 d . . . . . H3 H 0.515155 0.244957 -0.510234 0.045 Uiso 1 1 calc R U . . . O1 O 0.27579(13) 0.20798(9) -0.37715(8) 0.03882(19) Uani 1 1 d . . . . . H1O H 0.216(3) 0.174(2) -0.3235(18) 0.061(5) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.0351(5) 0.0250(4) 0.0357(4) 0.0128(3) 0.0054(3) 0.0067(3) C2A 0.0294(4) 0.0288(4) 0.0349(4) 0.0144(3) 0.0064(3) 0.0052(3) C3A 0.0343(5) 0.0306(4) 0.0348(4) 0.0112(3) 0.0018(4) 0.0014(3) C4A 0.0385(5) 0.0250(4) 0.0415(5) 0.0107(4) 0.0059(4) 0.0027(3) F1A 0.0577(5) 0.0454(4) 0.0442(4) 0.0154(3) -0.0116(3) -0.0068(3) O1A 0.0555(5) 0.0319(4) 0.0399(4) 0.0142(3) -0.0052(3) 0.0047(3) N1A 0.0422(5) 0.0239(3) 0.0401(4) 0.0140(3) 0.0029(3) 0.0065(3) N2A 0.0374(4) 0.0239(3) 0.0358(4) 0.0132(3) 0.0031(3) 0.0054(3) N3A 0.0457(5) 0.0361(5) 0.0416(5) 0.0209(4) -0.0010(4) 0.0039(4) C1B 0.0356(4) 0.0251(4) 0.0296(4) 0.0135(3) 0.0089(3) 0.0060(3) C2B 0.0317(4) 0.0290(4) 0.0292(4) 0.0134(3) 0.0084(3) 0.0028(3) C3B 0.0396(5) 0.0369(5) 0.0288(4) 0.0167(4) 0.0033(3) 0.0041(4) C4B 0.0472(6) 0.0352(5) 0.0350(5) 0.0213(4) 0.0074(4) 0.0099(4) F1B 0.0703(5) 0.0527(4) 0.0367(4) 0.0213(3) -0.0100(3) -0.0022(4) O1B 0.0517(5) 0.0290(3) 0.0307(3) 0.0122(3) 0.0029(3) 0.0021(3) N1B 0.0477(5) 0.0251(3) 0.0341(4) 0.0153(3) 0.0061(3) 0.0065(3) N2B 0.0368(4) 0.0234(3) 0.0297(3) 0.0125(3) 0.0052(3) 0.0034(3) N3B 0.0469(5) 0.0303(4) 0.0349(4) 0.0118(3) 0.0018(4) -0.0030(4) C1 0.0443(5) 0.0339(5) 0.0439(5) 0.0220(4) 0.0168(4) 0.0079(4) C2 0.0357(4) 0.0290(4) 0.0297(4) 0.0136(3) 0.0056(3) 0.0060(3) C3 0.0466(6) 0.0293(4) 0.0436(5) 0.0201(4) 0.0141(4) 0.0074(4) O1 0.0494(5) 0.0351(4) 0.0394(4) 0.0182(3) 0.0159(3) 0.0149(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A C1A N2A 121.28(9) . . ? O1A C1A N1A 120.31(9) . . ? N2A C1A N1A 118.41(9) . . ? N2A C2A N3A 119.38(9) . . ? N2A C2A C3A 119.83(9) . . ? N3A C2A C3A 120.78(10) . . ? C4A C3A F1A 121.98(9) . . ? C4A C3A C2A 119.59(9) . . ? F1A C3A C2A 118.43(9) . . ? C3A C4A N1A 119.04(9) . . ? C3A C4A H4A 120.5 . . ? N1A C4A H4A 120.5 . . ? C4A N1A C1A 122.16(9) . . ? C4A N1A H4N 124.0(10) . . ? C1A N1A H4N 113.7(10) . . ? C2A N2A C1A 120.93(8) . . ? C2A N3A H5N 116.5(12) . . ? C2A N3A H6N 120.5(15) . . ? H5N N3A H6N 123.0(19) . . ? O1B C1B N2B 120.93(8) . . ? O1B C1B N1B 119.55(8) . . ? N2B C1B N1B 119.52(9) . . ? N3B C2B N2B 119.10(9) . . ? N3B C2B C3B 121.28(9) . . ? N2B C2B C3B 119.62(9) . . ? F1B C3B C4B 122.10(9) . . ? F1B C3B C2B 118.11(9) . . ? C4B C3B C2B 119.78(9) . . ? C3B C4B N1B 118.69(9) . . ? C3B C4B H4B 120.7 . . ? N1B C4B H4B 120.7 . . ? C4B N1B C1B 121.73(9) . . ? C4B N1B H1N 125.0(11) . . ? C1B N1B H1N 113.3(11) . . ? C2B N2B C1B 120.50(8) . . ? C2B N3B H2N 117.6(12) . . ? C2B N3B H3N 116.2(11) . . ? H2N N3B H3N 126.1(17) . . ? C3 C1 C2 119.86(9) 2_654 . ? C3 C1 H1 120.1 2_654 . ? C2 C1 H1 120.1 . . ? O1 C2 C3 117.17(9) . . ? O1 C2 C1 123.09(9) . . ? C3 C2 C1 119.74(9) . . ? C2 C3 C1 120.40(9) . 2_654 ? C2 C3 H3 119.8 . . ? C1 C3 H3 119.8 2_654 . ? C2 O1 H1O 109.7(12) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A O1A 1.2405(13) . ? C1A N2A 1.3625(12) . ? C1A N1A 1.3801(13) . ? C2A N2A 1.3288(13) . ? C2A N3A 1.3307(13) . ? C2A C3A 1.4234(14) . ? C3A C4A 1.3439(15) . ? C3A F1A 1.3481(12) . ? C4A N1A 1.3514(14) . ? C4A H4A 0.9300 . ? N1A H4N 0.947(14) . ? N3A H5N 0.89(2) . ? N3A H6N 0.793(19) . ? C1B O1B 1.2584(12) . ? C1B N2B 1.3486(12) . ? C1B N1B 1.3732(12) . ? C2B N3B 1.3262(13) . ? C2B N2B 1.3333(12) . ? C2B C3B 1.4249(14) . ? C3B F1B 1.3429(12) . ? C3B C4B 1.3447(16) . ? C4B N1B 1.3560(14) . ? C4B H4B 0.9300 . ? N1B H1N 0.940(14) . ? N3B H2N 0.793(17) . ? N3B H3N 0.897(18) . ? C1 C3 1.3875(16) 2_654 ? C1 C2 1.3901(14) . ? C1 H1 0.9300 . ? C2 O1 1.3791(13) . ? C2 C3 1.3845(14) . ? C3 H3 0.9300 . ? O1 H1O 0.90(2) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N3A H6N O1 0.793(19) 2.36(2) 3.0697(13) 149.7(19) 2_554 yes N3B H2N O1 0.793(17) 2.389(17) 3.0494(13) 141.5(16) 2_665 yes N3B H3N O1A 0.897(18) 1.979(19) 2.8745(14) 176.6(16) 1_565 yes C3 H3 F1B 0.93 2.62 3.3269(13) 133.5 1_554 yes N1A H4N N2B 0.947(14) 1.871(14) 2.8165(12) 175.7(15) 1_545 yes O1 H1O O1B 0.90(2) 1.81(2) 2.7081(11) 176.9(18) . yes N3A H5N O1B 0.89(2) 1.99(2) 2.8777(13) 172.9(17) . yes N1B H1N N2A 0.940(14) 1.852(15) 2.7913(12) 176.8(16) . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2A C2A C3A C4A -1.47(16) . . . . ? N3A C2A C3A C4A 179.06(11) . . . . ? N2A C2A C3A F1A 178.55(9) . . . . ? N3A C2A C3A F1A -0.91(16) . . . . ? F1A C3A C4A N1A -179.90(10) . . . . ? C2A C3A C4A N1A 0.13(17) . . . . ? C3A C4A N1A C1A 0.61(17) . . . . ? O1A C1A N1A C4A -179.52(10) . . . . ? N2A C1A N1A C4A -0.05(15) . . . . ? N3A C2A N2A C1A -178.45(10) . . . . ? C3A C2A N2A C1A 2.08(15) . . . . ? O1A C1A N2A C2A 178.14(10) . . . . ? N1A C1A N2A C2A -1.33(15) . . . . ? N3B C2B C3B F1B -0.28(15) . . . . ? N2B C2B C3B F1B -179.44(9) . . . . ? N3B C2B C3B C4B 178.97(10) . . . . ? N2B C2B C3B C4B -0.19(16) . . . . ? F1B C3B C4B N1B -178.90(10) . . . . ? C2B C3B C4B N1B 1.88(16) . . . . ? C3B C4B N1B C1B -0.26(16) . . . . ? O1B C1B N1B C4B 176.38(9) . . . . ? N2B C1B N1B C4B -3.13(15) . . . . ? N3B C2B N2B C1B 177.60(9) . . . . ? C3B C2B N2B C1B -3.23(14) . . . . ? O1B C1B N2B C2B -174.65(9) . . . . ? N1B C1B N2B C2B 4.85(14) . . . . ? C3 C1 C2 O1 179.09(10) 2_654 . . . ? C3 C1 C2 C3 0.13(19) 2_654 . . . ? O1 C2 C3 C1 -179.15(10) . . . 2_654 ? C1 C2 C3 C1 -0.13(19) . . . 2_654 ? _cod_database_fobs_code 2312702